The objective of this project is research on and development of new mass spectral techniques in order to provide innovative and/or more rapid solutions to problems involving (1) chemical structure determination, (2) complex mixture analysis and (3) measurement of trace components in biological systems. Electrospray ionization mass spectrometry, tandem mass spectrometry and combined liquid chromatography-mass spectrometry are the techniques of current interest. A rapid and sensitive analytical method utilizing on-line liquid chromatography-electrospray ionization- tandem mass spectrometry has been developed to measure the Phase I anti- AIDS clinical candidate 2'-beta-fluoro-2',3'-dideoxyadenosine in human plasma. Fast atom bombardment mass spectrometry has been used to characterize the structure of a series of hydroxylated aromatic inhibitors of HIV-1 integrase.